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GB/T 31854-2015 English PDF (GBT31854-2015)

GB/T 31854-2015 English PDF (GBT31854-2015)

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GB/T 31854-2015: Test method for measuring metallic impurities content in silicon materials used for photovoltaic applications by inductively coupled plasma mass spectrometry

This standard specifies a method for the determination of trace metal impurities in silicon materials for photovoltaic applications by inductively coupled plasma mass spectrometry (ICP-MS). This standard applies to the determination of trace metal impurities of iron, chromium, nickel, copper, zinc in silicon materials for photovoltaic applications.
GB/T 31854-2015
GB
NATIONAL STANDARD OF THE
PEOPLE REPUBLIC OF CHINA
ICS 29.045
H 82
Test method for measuring metallic impurities content
in silicon materials used for photovoltaic applications
by inductively coupled plasma mass spectrometry
ISSUED ON: JULY 03, 2015
IMPLEMENTED ON: MARCH 01, 2016
Issued by: General Administration of Quality Supervision, Inspection and Quarantine;
Standardization Administration of PRC.
Table of Contents
Foreword ... 3
1 Scope ... 4
2 Normative references ... 4
3 Method summary ... 5
4 Disturbing factors ... 5
5 Reagents ... 5
6 Apparatus and equipment ... 6
7 Environmental conditions ... 6
8 Specimen preparation ... 6
9 Test procedure ... 7
10 Results processing ... 9
11 Precision ... 9
12 Quality assurance and control ... 10
13 Report ... 10
Test method for measuring metallic impurities content
in silicon materials used for photovoltaic applications
by inductively coupled plasma mass spectrometry
Warning - The personnel using this standard shall have practical
experience in formal laboratory work. This standard does not point out all possible safety issues. The user is responsible for taking appropriate
safety and health measures and ensuring compliance with the conditions
stipulated by relevant national laws and regulations.
1 Scope
This standard specifies a method for the determination of trace metal impurities in silicon materials for photovoltaic applications by inductively coupled plasma mass spectrometry (ICP-MS).
This standard applies to the determination of trace metal impurities of iron, chromium, nickel, copper, zinc in silicon materials for photovoltaic applications. The measurement range of each element is as shown in Table 1.
2 Normative references
The following documents are essential to the application of this document. For the dated documents, only the versions with the dates indicated are applicable to this document; for the undated documents, only the latest version (including all the amendments) are applicable to this standard.
d) Standard storage solution: The concentrations of iron, chromium, nickel, copper, zinc, yttrium are all 1 mg/mL; certified reference materials that can be traced to the source at home and abroad are used;
e) Nitric acid solution: The volume ratio of nitric acid and ultrapure water is VHNO3:VH2O = 1:19;
f) Nitric acid-hydrofluoric acid mixed solution: The volume ratio of nitric acid and hydrofluoric acid is VHNO3:VHF = 1:2.
6 Apparatus and equipment
This method requires the following instruments and equipment:
a) Inductively coupled plasma mass spectrometer;
b) Analytical balance: The sensitivity is 0.1 mg;
c) Fume hood;
d) Utensils: The utensils used shall be made of polytetrafluoroethylene (PTFE) or perfluoroalkoxy resin (PFA) and other materials that are
resistant to hydrofluoric acid corrosion and can be cleaned;
e) Electric heating plate.
7 Environmental conditions
7.1 Temperature: 18 ??C ~ 25 ??C.
7.2 Relative humidity: It shall not be greater than 65%.
7.3 Cleanliness: It shall be better than the ISO level-6 cleanliness requirements as defined in GB/T 25915.1-2010.
8 Specimen preparation
8.1 Process the sample into particles that are easy to dissolve; it shall strictly avoid contamination during the crushing process.
8.2 Treat the specimen in an appropriate concentration of hydrofluoric acid solution; add an appropriate concentration of nitric acid solution if necessary; use ultrapure water to wash it.
8.3 Dry the specimen at 100 ??C ~ 110 ??C to prepare for use.
9.4.3 Preparation of yttrium standard solution
Pipette 100 ??L of yttrium standard stock solution; place it in a 100 mL volumetric flask; add 40 mL nitric acid solution; use ultrapure water to dilute it to the mark; shake it uniformly; the concentration of this standard solution is 1 ??g/mL. 9.4.4 Preparation of yttrium standard working solution
Pipette 200 ??L of yttrium standard solution in a 100 mL volumetric flask; add 40 mL of nitric acid solution; use ultrapure water to dilute it to the mark; shake it uniformly; the concentration of this standard solution is 2 ??g/mL.
9.5 Preparation of sample solution
Place the specimen in a clean, open container which has an appropriate volume; add an appropriate amount of nitric acid-hydrofluoric acid mixed solution according to Table 2; heat to dissolve the specimen; evaporate the solution at 160 ??C ~ 170 ??C to dry. After cooling at room temperature, add 4 mL of nitric acid-hydrofluoric acid mixed solution to dissolve the residue; then evaporate the solution to dryness again at 160 ??C ~ 170 ??C. Add 4 mL of nitric acid solution, shake well to dissolve the residue completely; transfer the solution to a 10 mL volumetric flask; use ultrapure water to make its volume to the mark; shake well; prepare for ICP-MS determination.
9.6 Instrumental analysis
9.6.1 Instrument preparation
Before the test, the inductively coupled plasma mass spectrometer needs to set proper working conditions and be tuned, to achieve the best test conditions. 9.6.2 Selection of isotope
The selection of the isotope of each element to be analyzed and the internal standard element in the sample shall be carried out according to Table 3. 9.6.3 Analysis
The blank solution, sample solution and standard series of working solutions

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